反应详情

温度

100 °C

Take up 4-[1,3]dioxolan-2-yl-2-methylphenol (Example 388, Part C2) (0.288 g, 2.06 mmol), 5-chloropyrazine-2-carbonitrile (0.372 g, 2.06 mmol) and K2CO3 (0.428 g 3.10 mmol) in DMF (13.8 mL). Heat at 100° C. for 45 minutes. Cool to 80° C. and stir overnight. Dilute the reaction mixture with dichloromethane (100 mL). Wash the organic layer with saturated aqueous NaBCO3 (2×25 mL) and brine (1×25 mL). Dry over Na2CO3, filter and concentrate. Purify by flash chromatography, eluting with 30% ethyl acetate in hexanes to give the title compound (0.560 g, 95.58%): TLC [silica gel 60 F254, 30% ethyl acetate in hexanes] Rf=0.52.

1. temperatureCool to 80° C.
2. washWash the organic layer with saturated aqueous NaBCO3 (2×25 mL) and brine (1×25 mL)
3. dry with materialDry over Na2CO3
4. filtrationfilter
5. concentrationconcentrate
6. customPurify by flash chromatography
7. washeluting with 30% ethyl acetate in hexanes